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Author: Subject: Preparation of elemental phosphorus
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[*] posted on 5-12-2011 at 18:38


what happens when all your water has turned to steam?



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shannon dove
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[*] posted on 6-12-2011 at 05:43


The ultra fine mist would come down from the top of the jar and pass through the arc then it would condense on the bottom of the jar , and be pumped back to the mister and cycle again.
For the phosphate liquid-mist, what about water soluble phosphate dissolved in water and alchohol mixture. At arc temperature the carbon in the ethanal will combine with the oxygen in the phosphate. I know at arc temps the ethanal will not be ethanal anymore, but whatever organic compounds are formed , the carbon should still be able to reduce phosphates and form carbon monoxide. I think at arc temps the e
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[*] posted on 6-12-2011 at 06:21


At arc temps the alcahol will form lampblack type carbon and free hydrogen and the oxygen atom in alcahol will just unite with the hydrogen, maybe some acetalyne will be formed (charcoal and hydrogen react in an arc to form acetalyne).
In this closed system there will be a whole lot of unreacted alcahol and I think there might form some very complicated organic phosphorus compounds, but these should break down in the arc and make phosphine, and I think from phosphine we could easily get phosphorus.
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[*] posted on 6-12-2011 at 08:18


Quote: Originally posted by blogfast25  
shannon dove:

Hydrogen cannot reduce phosphates or P2O5, not by a long shot.

Your idea cannot work, period.


It appears that hydrogen can in fact reduce phosphates: http://pubs.acs.org/doi/abs/10.1021/cm970175g

And I quote -Several transition-metal phosphates, arsenates, and antimonates undergo direct reduction in hydrogen at relatively low temperatures (400−1050 °C) to the corresponding phosphides, arsenides, and antimonides....., and -We could not however synthesize pnictides of manganese, vanadium, and gallium by this route, suggesting that the method is applicable only to those metals that are less electropositive than hydrogen, that is, those metals whose binary oxides are reducible by hydrogen to the metallic state.




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[*] posted on 6-12-2011 at 08:45


Quote: Originally posted by shannon dove  
At arc temps the alcahol will form lampblack type carbon and free hydrogen and the oxygen atom in alcahol will just unite with the hydrogen, maybe some acetalyne will be formed (charcoal and hydrogen react in an arc to form acetalyne).
In this closed system there will be a whole lot of unreacted alcahol and I think there might form some very complicated organic phosphorus compounds, but these should break down in the arc and make phosphine, and I think from phosphine we could easily get phosphorus.


This sounds like a novel way to have a nasty and to an observer at a safe distance interesting accident.
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[*] posted on 6-12-2011 at 11:19


iron oxide is reduced to metal by hydrogen, so iron phosphate should be reduced to iron phosphide by hydrogen. What if we dissolve tricalcium phosphate in hydrochloric acid, then add iron chloride to precipitate iron phosphate, heat iron phosphate to dull red in hydrogen to get iron phosphide, react this phosphide with hydrochloric acid to make phosphine. I think iron phosphide reacts very slowly with acids , so it should be ground to a fine powder first.
I know, I know, something simular to this has already been talked about on this thread, but there was not much talk about the best way to make iron phosphide and more important the temperature needed.
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[*] posted on 6-12-2011 at 12:59


Quote: Originally posted by bahamuth  


It appears that hydrogen can in fact reduce phosphates: http://pubs.acs.org/doi/abs/10.1021/cm970175g



Your link and quote say nothing about how this is achieved.

Quote: Originally posted by shannon dove  
iron oxide is reduced to metal by hydrogen, so iron phosphate should be reduced to iron phosphide by hydrogen.


And you conclude this, how???

For instance, iron (III) phosphate’s structure is that of ferric ions, Fe<sup>3+</sup> and phosphate ions, PO<sub>4</sub><sup>3-</sup>, joined in an ionic lattice. Reduction with hydrogen here is very similar to reducing P2O5 with hydrogen and that cannot be done because P2O5 has far too high a heat of formation.

In bahamuth’s linked paper undoubtedly forcing conditions are applied to reduce D-block phosphates to phosphides.




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[*] posted on 6-12-2011 at 14:12


Aluminum oxide , silicon dioxide and calcium oxide all have very very high heat of formation, but from the books I have read, under certain conditions, all can be reduced by carbon in an electric furnace. I know that early attemps to do this with calcium only made calcium carbide, but I have also read that it has been done.
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[*] posted on 6-12-2011 at 14:42


Quote: Originally posted by shannon dove  
Aluminum oxide , silicon dioxide and calcium oxide all have very very high heat of formation, but from the books I have read, under certain conditions, all can be reduced by carbon in an electric furnace. I know that early attemps to do this with calcium only made calcium carbide, but I have also read that it has been done.


These are reduced because one of the gaseous reaction products (CO or CO2) is removed from the mix, that pushes the equilibrium to the right. using hydrogen that's not possible because it is a gas itself. In the case of Calcium, that too can be distilled off.

You're flogging a dead horse here...




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[*] posted on 6-12-2011 at 14:50


Forget I said anything about hydrogen, maybe I am wrong, thats why I ask people on here, to see if my ideas sound possible before I waste a lot of time and money on an impossible project. I will give up on reducing phosphates with hydrogen.
Anyway, I have been searching for hours on methods of making iron phosphide. I have been searching patents. Does this sound possible, I drop a spoonfull of iron phosphide powder into a jar half filled with acid, a tube made into the top tranfers the phosphine to a pipe heated to about 600 celcius, the phosphine deposits phosphorus.
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[*] posted on 7-12-2011 at 09:03


Quote: Originally posted by shannon dove  
Does this sound possible, I drop a spoonfull of iron phosphide powder into a jar half filled with acid, a tube made into the top tranfers the phosphine to a pipe heated to about 600 celcius, the phosphine deposits phosphorus.


Phosphine(s) are very dangerous: highly flammable and highly toxic. Really not something you want to mess with in appreciable quantities in a makeshift home lab.

Producing phosphorus in home lab attainable conditions isn’t really that hard. But capturing the formed P is harder, as this whole thread testifies to. For home chemists the reaction of sodium metaphosphate with aluminium powder and silica remains the most viable option.




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[*] posted on 8-12-2011 at 06:18


This is just my opinion, please do not get mad.
Using aluminium for any home chemical project is cheating ! Aluminium is more difficult to make than phosphorus. Using aluminium to make phosphorus is like buying red phosphorus then turning it into white phosphorus and bragging that you made white phosphorus. Its like getting someone else to make you some concentrated nitric acid and glycerin, then bragging that you made nitroglycerine.
If you use aluminium, the aluminium factory has done three/quarters of the work for you. Any post that talks about using aluminium, I do not even read it.
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[*] posted on 8-12-2011 at 06:34


Home chemistry is about using what you can get your hands on. If you call that 'cheating' you're unlikely to ever make anything at home, unless you're a well equipped near-genius with far too much time on his hands.

If I read you correctly, for instance someone using zinc/carbon battery fill to extract MnSO4 would be cheating because he's using existing batteries and didn't go and mine some sulphur and turn it into sulphuric acid? Or extract his own oxalic acid from rhubarb?

What you say is absurd!





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[*] posted on 8-12-2011 at 06:47


Quote: Originally posted by shannon dove  
Forget I said anything about hydrogen, maybe I am wrong, thats why I ask people on here, to see if my ideas sound possible before I waste a lot of time and money on an impossible project. I will give up on reducing phosphates with hydrogen.
Anyway, I have been searching for hours on methods of making iron phosphide. I have been searching patents. Does this sound possible, I drop a spoonfull of iron phosphide powder into a jar half filled with acid, a tube made into the top tranfers the phosphine to a pipe heated to about 600 celcius, the phosphine deposits phosphorus.


It sounds like an excellent way of making a a sizable explosion that will spray you with glass, acid and toxic shit.
Most lab chemistry, even real professional labs, uses methods and reagents that are different to industrial methods and use premade reagents a lot of the time.
Aluminium is cheaply and readily available compared to phosphorous as far as home chemists are concerned so it is a viable reagent for them.
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[*] posted on 8-12-2011 at 07:05


But you could make sulphuric acid at home if you had to, but aluminium on the other hand would be a hundred times more difficult.
I am just saying I would feel a lot more of an accomplishment if I did not use a ready made off the shelf very strong reducer like aluminium. Aluminium will pull the oxygen out of anything!! (almost).
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[*] posted on 8-12-2011 at 07:41


Quote: Originally posted by shannon dove  
Aluminium will pull the oxygen out of anything!! (almost).


Yes but it turns out that recovering the reduced phosphorus really is the hard part at home level!




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[*] posted on 8-12-2011 at 08:12


Ok, those are all good points.
I have been thinking about doing the well tested method of reducing phosphates with aluminium.
I will still look for other methods too.
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[*] posted on 8-12-2011 at 08:42


Quote: Originally posted by blogfast25  
Quote: Originally posted by shannon dove  
Aluminium will pull the oxygen out of anything!! (almost).


Yes but it turns out that recovering the reduced phosphorus really is the hard part at home level!


Together with not setting fire to or poisoning yourself with the bastard stuff.
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[*] posted on 12-12-2011 at 11:16


yes please let us know how it works out for you i am dying to find out!
i want to use sodium tri phosphate from home depot . dehydrate the stp in the oven before mixing with sillica and active carbon all of the above in a small steel tube , the latest in the grill with air blowing on the hot charcoal....should be enough heat....hopefully .
a copper tube is leading the gasses in a cold bucket of water...

my concern ( other than not getting phosphorus) is the presence of sulfates in the original stp...?
the box doesnt give any info ..
any thought?
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[*] posted on 12-12-2011 at 15:16


You said trisodium phosphate, silica and charcoal; what about aluminum powder?
Read the rest of this thread. It seems that aluminium works at a lower temp, so its better for backyard chemist.
It will be a while before I try it, I still have to make a propane torch or furnace.
I am thinking air blast from leaf blower plus propane.
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[*] posted on 12-12-2011 at 15:34


I realy realy realy wish that charcoal woul work instead of aluminium!!!
Just like I realy wish that dilute nitric acid would nitrate stuff !!!
The many challenges of chemistry.
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[*] posted on 13-12-2011 at 05:56


Quote: Originally posted by neptunium  
dehydrate the stp in the oven before mixing with sillica and active carbon all of the above in a small steel tube , the latest in the grill with air blowing on the hot charcoal....should be enough heat....?


The heat you need to carry this off with carbon will soften your steel.

Use hexasodiummetaphosphate ((NaPO3)6, HSMP) and aluminium powder (and silica) instead. Read the thread for sources of HSMP. And check out the safety precautions: phosphorus is a dangerous substance!!!

[Edited on 13-12-2011 by blogfast25]




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[*] posted on 13-12-2011 at 06:53


i was just thinking of activated carbon because thats what i have right here but aluminum powder is a VERY usefull reducing agent indeed and if order some i will absolutlytry it !!
I used to collect samples of each elements and had played with both red and white phosphorus back when it didnt raised any flags (thank you DHS and DEA)....ha that takes me back !....good times!
Also i wanted to continuously flush the tube with a low flow of argon ,to prevent any suck back of water ... i dont really want to open a hot steel tube full of hot white P!
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[*] posted on 13-12-2011 at 07:00


Use hexasodiummetaphosphate ((NaPO3)6, HSMP)...good idea! melting point 550C...most of the one i've found contain sodium carbonate though
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[*] posted on 13-12-2011 at 10:03


Quote: Originally posted by neptunium  
Use hexasodiummetaphosphate ((NaPO3)6, HSMP)...good idea! melting point 550C...most of the one i've found contain sodium carbonate though


A bit of carbonate won't hurt here.




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